CN115627163B - 一种高荧光量子产率紫光钙钛矿量子点的制备方法 - Google Patents
一种高荧光量子产率紫光钙钛矿量子点的制备方法 Download PDFInfo
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- 239000002096 quantum dot Substances 0.000 title claims abstract description 109
- 238000006862 quantum yield reaction Methods 0.000 title claims abstract description 32
- 238000002360 preparation method Methods 0.000 title claims abstract description 14
- 239000002243 precursor Substances 0.000 claims abstract description 36
- 239000000243 solution Substances 0.000 claims abstract description 30
- 239000002904 solvent Substances 0.000 claims abstract description 30
- 239000007788 liquid Substances 0.000 claims abstract description 27
- HWSZZLVAJGOAAY-UHFFFAOYSA-L lead(II) chloride Chemical compound Cl[Pb]Cl HWSZZLVAJGOAAY-UHFFFAOYSA-L 0.000 claims abstract description 25
- 229910052792 caesium Inorganic materials 0.000 claims abstract description 24
- TVFDJXOCXUVLDH-UHFFFAOYSA-N caesium atom Chemical class [Cs] TVFDJXOCXUVLDH-UHFFFAOYSA-N 0.000 claims abstract description 24
- 239000003446 ligand Substances 0.000 claims abstract description 21
- 238000000034 method Methods 0.000 claims abstract description 15
- 239000011261 inert gas Substances 0.000 claims abstract description 10
- 239000000654 additive Substances 0.000 claims abstract description 9
- 230000000996 additive effect Effects 0.000 claims abstract description 9
- 150000003841 chloride salts Chemical class 0.000 claims abstract description 9
- 239000013110 organic ligand Substances 0.000 claims abstract description 9
- 238000002156 mixing Methods 0.000 claims abstract description 6
- 238000010438 heat treatment Methods 0.000 claims abstract description 4
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 claims description 54
- XEKOWRVHYACXOJ-UHFFFAOYSA-N Ethyl acetate Chemical compound CCOC(C)=O XEKOWRVHYACXOJ-UHFFFAOYSA-N 0.000 claims description 45
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 20
- 238000003756 stirring Methods 0.000 claims description 18
- 239000011550 stock solution Substances 0.000 claims description 16
- WRIDQFICGBMAFQ-UHFFFAOYSA-N (E)-8-Octadecenoic acid Natural products CCCCCCCCCC=CCCCCCCC(O)=O WRIDQFICGBMAFQ-UHFFFAOYSA-N 0.000 claims description 12
- LQJBNNIYVWPHFW-UHFFFAOYSA-N 20:1omega9c fatty acid Natural products CCCCCCCCCCC=CCCCCCCCC(O)=O LQJBNNIYVWPHFW-UHFFFAOYSA-N 0.000 claims description 12
- QSBYPNXLFMSGKH-UHFFFAOYSA-N 9-Heptadecensaeure Natural products CCCCCCCC=CCCCCCCCC(O)=O QSBYPNXLFMSGKH-UHFFFAOYSA-N 0.000 claims description 12
- 239000005642 Oleic acid Substances 0.000 claims description 12
- ZQPPMHVWECSIRJ-UHFFFAOYSA-N Oleic acid Natural products CCCCCCCCC=CCCCCCCCC(O)=O ZQPPMHVWECSIRJ-UHFFFAOYSA-N 0.000 claims description 12
- QXJSBBXBKPUZAA-UHFFFAOYSA-N isooleic acid Natural products CCCCCCCC=CCCCCCCCCC(O)=O QXJSBBXBKPUZAA-UHFFFAOYSA-N 0.000 claims description 12
- CCCMONHAUSKTEQ-UHFFFAOYSA-N octadecene Natural products CCCCCCCCCCCCCCCCC=C CCCMONHAUSKTEQ-UHFFFAOYSA-N 0.000 claims description 12
- ZQPPMHVWECSIRJ-KTKRTIGZSA-N oleic acid Chemical compound CCCCCCCC\C=C/CCCCCCCC(O)=O ZQPPMHVWECSIRJ-KTKRTIGZSA-N 0.000 claims description 12
- 239000002244 precipitate Substances 0.000 claims description 12
- 229910052757 nitrogen Inorganic materials 0.000 claims description 10
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 8
- VLKZOEOYAKHREP-UHFFFAOYSA-N n-Hexane Chemical compound CCCCCC VLKZOEOYAKHREP-UHFFFAOYSA-N 0.000 claims description 7
- UHOVQNZJYSORNB-UHFFFAOYSA-N Benzene Chemical compound C1=CC=CC=C1 UHOVQNZJYSORNB-UHFFFAOYSA-N 0.000 claims description 6
- 125000000129 anionic group Chemical group 0.000 claims description 6
- FJDQFPXHSGXQBY-UHFFFAOYSA-L caesium carbonate Chemical compound [Cs+].[Cs+].[O-]C([O-])=O FJDQFPXHSGXQBY-UHFFFAOYSA-L 0.000 claims description 6
- 229910000024 caesium carbonate Inorganic materials 0.000 claims description 6
- 125000002091 cationic group Chemical group 0.000 claims description 6
- RMZAYIKUYWXQPB-UHFFFAOYSA-N trioctylphosphane Chemical compound CCCCCCCCP(CCCCCCCC)CCCCCCCC RMZAYIKUYWXQPB-UHFFFAOYSA-N 0.000 claims description 6
- DKIDEFUBRARXTE-UHFFFAOYSA-N 3-mercaptopropanoic acid Chemical compound OC(=O)CCS DKIDEFUBRARXTE-UHFFFAOYSA-N 0.000 claims description 5
- DTRIDVOOPAQEEL-UHFFFAOYSA-N 4-sulfanylbutanoic acid Chemical compound OC(=O)CCCS DTRIDVOOPAQEEL-UHFFFAOYSA-N 0.000 claims description 4
- 229910052786 argon Inorganic materials 0.000 claims description 4
- FLJPGEWQYJVDPF-UHFFFAOYSA-L caesium sulfate Chemical compound [Cs+].[Cs+].[O-]S([O-])(=O)=O FLJPGEWQYJVDPF-UHFFFAOYSA-L 0.000 claims description 4
- 238000001816 cooling Methods 0.000 claims description 4
- IOQPZZOEVPZRBK-UHFFFAOYSA-N octan-1-amine Chemical compound CCCCCCCCN IOQPZZOEVPZRBK-UHFFFAOYSA-N 0.000 claims description 4
- TVMXDCGIABBOFY-UHFFFAOYSA-N octane Chemical compound CCCCCCCC TVMXDCGIABBOFY-UHFFFAOYSA-N 0.000 claims description 4
- 239000002245 particle Substances 0.000 claims description 3
- 229910001631 strontium chloride Inorganic materials 0.000 claims description 3
- AHBGXTDRMVNFER-UHFFFAOYSA-L strontium dichloride Chemical group [Cl-].[Cl-].[Sr+2] AHBGXTDRMVNFER-UHFFFAOYSA-L 0.000 claims description 3
- XDTMQSROBMDMFD-UHFFFAOYSA-N Cyclohexane Chemical compound C1CCCCC1 XDTMQSROBMDMFD-UHFFFAOYSA-N 0.000 claims description 2
- XBDQKXXYIPTUBI-UHFFFAOYSA-M Propionate Chemical compound CCC([O-])=O XBDQKXXYIPTUBI-UHFFFAOYSA-M 0.000 claims description 2
- KXKVLQRXCPHEJC-UHFFFAOYSA-N acetic acid trimethyl ester Natural products COC(C)=O KXKVLQRXCPHEJC-UHFFFAOYSA-N 0.000 claims description 2
- ZOAIGCHJWKDIPJ-UHFFFAOYSA-M caesium acetate Chemical compound [Cs+].CC([O-])=O ZOAIGCHJWKDIPJ-UHFFFAOYSA-M 0.000 claims description 2
- WLZGEDNSZCPRCJ-UHFFFAOYSA-M cesium;octadecanoate Chemical compound [Cs+].CCCCCCCCCCCCCCCCCC([O-])=O WLZGEDNSZCPRCJ-UHFFFAOYSA-M 0.000 claims description 2
- HEQUOWMMDQTGCX-UHFFFAOYSA-L dicesium;oxalate Chemical compound [Cs+].[Cs+].[O-]C(=O)C([O-])=O HEQUOWMMDQTGCX-UHFFFAOYSA-L 0.000 claims description 2
- 150000004820 halides Chemical class 0.000 claims description 2
- 239000005457 ice water Substances 0.000 claims description 2
- 239000011259 mixed solution Substances 0.000 claims description 2
- 239000000203 mixture Substances 0.000 claims description 2
- 238000004020 luminiscence type Methods 0.000 abstract description 7
- 239000000463 material Substances 0.000 abstract description 5
- 230000004048 modification Effects 0.000 abstract description 2
- 238000012986 modification Methods 0.000 abstract description 2
- NCMHKCKGHRPLCM-UHFFFAOYSA-N caesium(1+) Chemical compound [Cs+] NCMHKCKGHRPLCM-UHFFFAOYSA-N 0.000 abstract 1
- 239000012045 crude solution Substances 0.000 abstract 1
- 238000005119 centrifugation Methods 0.000 description 11
- 239000010949 copper Substances 0.000 description 8
- 239000006185 dispersion Substances 0.000 description 7
- 238000005086 pumping Methods 0.000 description 7
- JJMDCOVWQOJGCB-UHFFFAOYSA-N 5-aminopentanoic acid Chemical compound [NH3+]CCCCC([O-])=O JJMDCOVWQOJGCB-UHFFFAOYSA-N 0.000 description 6
- 239000000047 product Substances 0.000 description 6
- GQEZCXVZFLOKMC-UHFFFAOYSA-N 1-hexadecene Chemical compound CCCCCCCCCCCCCCC=C GQEZCXVZFLOKMC-UHFFFAOYSA-N 0.000 description 4
- HFDVRLIODXPAHB-UHFFFAOYSA-N 1-tetradecene Chemical compound CCCCCCCCCCCCC=C HFDVRLIODXPAHB-UHFFFAOYSA-N 0.000 description 4
- WCUXLLCKKVVCTQ-UHFFFAOYSA-M Potassium chloride Chemical compound [Cl-].[K+] WCUXLLCKKVVCTQ-UHFFFAOYSA-M 0.000 description 4
- SNRUBQQJIBEYMU-UHFFFAOYSA-N dodecane Chemical compound CCCCCCCCCCCC SNRUBQQJIBEYMU-UHFFFAOYSA-N 0.000 description 4
- WWZKQHOCKIZLMA-UHFFFAOYSA-N octanoic acid Chemical compound CCCCCCCC(O)=O WWZKQHOCKIZLMA-UHFFFAOYSA-N 0.000 description 4
- QGLWBTPVKHMVHM-KTKRTIGZSA-N (z)-octadec-9-en-1-amine Chemical compound CCCCCCCC\C=C/CCCCCCCCN QGLWBTPVKHMVHM-KTKRTIGZSA-N 0.000 description 3
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 description 3
- MUBZPKHOEPUJKR-UHFFFAOYSA-N Oxalic acid Chemical compound OC(=O)C(O)=O MUBZPKHOEPUJKR-UHFFFAOYSA-N 0.000 description 3
- 235000005811 Viola adunca Nutrition 0.000 description 3
- 240000009038 Viola odorata Species 0.000 description 3
- 235000013487 Viola odorata Nutrition 0.000 description 3
- 235000002254 Viola papilionacea Nutrition 0.000 description 3
- 244000172533 Viola sororia Species 0.000 description 3
- 238000012512 characterization method Methods 0.000 description 3
- KBOPZPXVLCULAV-UHFFFAOYSA-N mesalamine Chemical compound NC1=CC=C(O)C(C(O)=O)=C1 KBOPZPXVLCULAV-UHFFFAOYSA-N 0.000 description 3
- 229960004963 mesalazine Drugs 0.000 description 3
- 239000012716 precipitator Substances 0.000 description 3
- 239000007787 solid Substances 0.000 description 3
- PAYRUJLWNCNPSJ-UHFFFAOYSA-N Aniline Chemical compound NC1=CC=CC=C1 PAYRUJLWNCNPSJ-UHFFFAOYSA-N 0.000 description 2
- VEXZGXHMUGYJMC-UHFFFAOYSA-M Chloride anion Chemical compound [Cl-] VEXZGXHMUGYJMC-UHFFFAOYSA-M 0.000 description 2
- ZAMOUSCENKQFHK-UHFFFAOYSA-N Chlorine atom Chemical compound [Cl] ZAMOUSCENKQFHK-UHFFFAOYSA-N 0.000 description 2
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 description 2
- 235000021355 Stearic acid Nutrition 0.000 description 2
- 238000010521 absorption reaction Methods 0.000 description 2
- OBETXYAYXDNJHR-UHFFFAOYSA-N alpha-ethylcaproic acid Natural products CCCCC(CC)C(O)=O OBETXYAYXDNJHR-UHFFFAOYSA-N 0.000 description 2
- 230000015572 biosynthetic process Effects 0.000 description 2
- 239000000460 chlorine Substances 0.000 description 2
- 229910052801 chlorine Inorganic materials 0.000 description 2
- ORTQZVOHEJQUHG-UHFFFAOYSA-L copper(II) chloride Chemical compound Cl[Cu]Cl ORTQZVOHEJQUHG-UHFFFAOYSA-L 0.000 description 2
- 230000007547 defect Effects 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- POULHZVOKOAJMA-UHFFFAOYSA-N dodecanoic acid Chemical compound CCCCCCCCCCCC(O)=O POULHZVOKOAJMA-UHFFFAOYSA-N 0.000 description 2
- VAMFXQBUQXONLZ-UHFFFAOYSA-N icos-1-ene Chemical compound CCCCCCCCCCCCCCCCCCC=C VAMFXQBUQXONLZ-UHFFFAOYSA-N 0.000 description 2
- CBFCDTFDPHXCNY-UHFFFAOYSA-N icosane Chemical compound CCCCCCCCCCCCCCCCCCCC CBFCDTFDPHXCNY-UHFFFAOYSA-N 0.000 description 2
- KWGKDLIKAYFUFQ-UHFFFAOYSA-M lithium chloride Chemical compound [Li+].[Cl-] KWGKDLIKAYFUFQ-UHFFFAOYSA-M 0.000 description 2
- QIQXTHQIDYTFRH-UHFFFAOYSA-N octadecanoic acid Chemical compound CCCCCCCCCCCCCCCCCC(O)=O QIQXTHQIDYTFRH-UHFFFAOYSA-N 0.000 description 2
- OQCDKBAXFALNLD-UHFFFAOYSA-N octadecanoic acid Natural products CCCCCCCC(C)CCCCCCCCC(O)=O OQCDKBAXFALNLD-UHFFFAOYSA-N 0.000 description 2
- 239000001103 potassium chloride Substances 0.000 description 2
- 235000011164 potassium chloride Nutrition 0.000 description 2
- FGDZQCVHDSGLHJ-UHFFFAOYSA-M rubidium chloride Chemical compound [Cl-].[Rb+] FGDZQCVHDSGLHJ-UHFFFAOYSA-M 0.000 description 2
- 239000008117 stearic acid Substances 0.000 description 2
- 238000003786 synthesis reaction Methods 0.000 description 2
- 229940095068 tetradecene Drugs 0.000 description 2
- ZMBHCYHQLYEYDV-UHFFFAOYSA-N trioctylphosphine oxide Chemical compound CCCCCCCCP(=O)(CCCCCCCC)CCCCCCCC ZMBHCYHQLYEYDV-UHFFFAOYSA-N 0.000 description 2
- JIAARYAFYJHUJI-UHFFFAOYSA-L zinc dichloride Chemical compound [Cl-].[Cl-].[Zn+2] JIAARYAFYJHUJI-UHFFFAOYSA-L 0.000 description 2
- PSBDWGZCVUAZQS-UHFFFAOYSA-N (dimethylsulfonio)acetate Chemical compound C[S+](C)CC([O-])=O PSBDWGZCVUAZQS-UHFFFAOYSA-N 0.000 description 1
- GYSCBCSGKXNZRH-UHFFFAOYSA-N 1-benzothiophene-2-carboxamide Chemical compound C1=CC=C2SC(C(=O)N)=CC2=C1 GYSCBCSGKXNZRH-UHFFFAOYSA-N 0.000 description 1
- RUFPHBVGCFYCNW-UHFFFAOYSA-N 1-naphthylamine Chemical compound C1=CC=C2C(N)=CC=CC2=C1 RUFPHBVGCFYCNW-UHFFFAOYSA-N 0.000 description 1
- FRPZMMHWLSIFAZ-UHFFFAOYSA-N 10-undecenoic acid Chemical compound OC(=O)CCCCCCCCC=C FRPZMMHWLSIFAZ-UHFFFAOYSA-N 0.000 description 1
- WBIQQQGBSDOWNP-UHFFFAOYSA-N 2-dodecylbenzenesulfonic acid Chemical compound CCCCCCCCCCCCC1=CC=CC=C1S(O)(=O)=O WBIQQQGBSDOWNP-UHFFFAOYSA-N 0.000 description 1
- UXVMQQNJUSDDNG-UHFFFAOYSA-L Calcium chloride Chemical compound [Cl-].[Cl-].[Ca+2] UXVMQQNJUSDDNG-UHFFFAOYSA-L 0.000 description 1
- GHVNFZFCNZKVNT-UHFFFAOYSA-N Decanoic acid Natural products CCCCCCCCCC(O)=O GHVNFZFCNZKVNT-UHFFFAOYSA-N 0.000 description 1
- MHZGKXUYDGKKIU-UHFFFAOYSA-N Decylamine Chemical compound CCCCCCCCCCN MHZGKXUYDGKKIU-UHFFFAOYSA-N 0.000 description 1
- 229910021578 Iron(III) chloride Inorganic materials 0.000 description 1
- 239000005639 Lauric acid Substances 0.000 description 1
- 229910021380 Manganese Chloride Inorganic materials 0.000 description 1
- GLFNIEUTAYBVOC-UHFFFAOYSA-L Manganese chloride Chemical compound Cl[Mn]Cl GLFNIEUTAYBVOC-UHFFFAOYSA-L 0.000 description 1
- 229910021586 Nickel(II) chloride Inorganic materials 0.000 description 1
- 238000002441 X-ray diffraction Methods 0.000 description 1
- 150000001413 amino acids Chemical class 0.000 description 1
- 230000005540 biological transmission Effects 0.000 description 1
- HQABUPZFAYXKJW-UHFFFAOYSA-N butan-1-amine Chemical compound CCCCN HQABUPZFAYXKJW-UHFFFAOYSA-N 0.000 description 1
- 239000001110 calcium chloride Substances 0.000 description 1
- 229910001628 calcium chloride Inorganic materials 0.000 description 1
- KHAVLLBUVKBTBG-UHFFFAOYSA-N caproleic acid Natural products OC(=O)CCCCCCCC=C KHAVLLBUVKBTBG-UHFFFAOYSA-N 0.000 description 1
- 230000015556 catabolic process Effects 0.000 description 1
- VYLVYHXQOHJDJL-UHFFFAOYSA-K cerium trichloride Chemical compound Cl[Ce](Cl)Cl VYLVYHXQOHJDJL-UHFFFAOYSA-K 0.000 description 1
- 150000001804 chlorine Chemical class 0.000 description 1
- 238000006731 degradation reaction Methods 0.000 description 1
- XRWMGCFJVKDVMD-UHFFFAOYSA-M didodecyl(dimethyl)azanium;bromide Chemical compound [Br-].CCCCCCCCCCCC[N+](C)(C)CCCCCCCCCCCC XRWMGCFJVKDVMD-UHFFFAOYSA-M 0.000 description 1
- LAWOZCWGWDVVSG-UHFFFAOYSA-N dioctylamine Chemical compound CCCCCCCCNCCCCCCCC LAWOZCWGWDVVSG-UHFFFAOYSA-N 0.000 description 1
- GPAYUJZHTULNBE-UHFFFAOYSA-N diphenylphosphine Chemical compound C=1C=CC=CC=1PC1=CC=CC=C1 GPAYUJZHTULNBE-UHFFFAOYSA-N 0.000 description 1
- 229940060296 dodecylbenzenesulfonic acid Drugs 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- NNMXSTWQJRPBJZ-UHFFFAOYSA-K europium(iii) chloride Chemical compound Cl[Eu](Cl)Cl NNMXSTWQJRPBJZ-UHFFFAOYSA-K 0.000 description 1
- 229910052736 halogen Inorganic materials 0.000 description 1
- 238000005286 illumination Methods 0.000 description 1
- PSCMQHVBLHHWTO-UHFFFAOYSA-K indium(iii) chloride Chemical compound Cl[In](Cl)Cl PSCMQHVBLHHWTO-UHFFFAOYSA-K 0.000 description 1
- RBTARNINKXHZNM-UHFFFAOYSA-K iron trichloride Chemical compound Cl[Fe](Cl)Cl RBTARNINKXHZNM-UHFFFAOYSA-K 0.000 description 1
- 239000011565 manganese chloride Substances 0.000 description 1
- 235000002867 manganese chloride Nutrition 0.000 description 1
- 229940099607 manganese chloride Drugs 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 229910001510 metal chloride Inorganic materials 0.000 description 1
- PXSXRABJBXYMFT-UHFFFAOYSA-N n-hexylhexan-1-amine Chemical compound CCCCCCNCCCCCC PXSXRABJBXYMFT-UHFFFAOYSA-N 0.000 description 1
- ATINCSYRHURBSP-UHFFFAOYSA-K neodymium(iii) chloride Chemical compound Cl[Nd](Cl)Cl ATINCSYRHURBSP-UHFFFAOYSA-K 0.000 description 1
- QMMRZOWCJAIUJA-UHFFFAOYSA-L nickel dichloride Chemical compound Cl[Ni]Cl QMMRZOWCJAIUJA-UHFFFAOYSA-L 0.000 description 1
- 235000021313 oleic acid Nutrition 0.000 description 1
- 235000006408 oxalic acid Nutrition 0.000 description 1
- -1 rare earth chloride salts Chemical class 0.000 description 1
- 229910052761 rare earth metal Inorganic materials 0.000 description 1
- 230000001105 regulatory effect Effects 0.000 description 1
- 229940102127 rubidium chloride Drugs 0.000 description 1
- BHXBZLPMVFUQBQ-UHFFFAOYSA-K samarium(iii) chloride Chemical compound Cl[Sm](Cl)Cl BHXBZLPMVFUQBQ-UHFFFAOYSA-K 0.000 description 1
- 239000011780 sodium chloride Substances 0.000 description 1
- 230000003595 spectral effect Effects 0.000 description 1
- 238000001228 spectrum Methods 0.000 description 1
- 229940117986 sulfobetaine Drugs 0.000 description 1
- GFISHBQNVWAVFU-UHFFFAOYSA-K terbium(iii) chloride Chemical compound Cl[Tb](Cl)Cl GFISHBQNVWAVFU-UHFFFAOYSA-K 0.000 description 1
- YBRBMKDOPFTVDT-UHFFFAOYSA-N tert-butylamine Chemical compound CC(C)(C)N YBRBMKDOPFTVDT-UHFFFAOYSA-N 0.000 description 1
- 230000001988 toxicity Effects 0.000 description 1
- 231100000419 toxicity Toxicity 0.000 description 1
- TUQOTMZNTHZOKS-UHFFFAOYSA-N tributylphosphine Chemical compound CCCCP(CCCC)CCCC TUQOTMZNTHZOKS-UHFFFAOYSA-N 0.000 description 1
- 229960002703 undecylenic acid Drugs 0.000 description 1
- 239000002699 waste material Substances 0.000 description 1
- CKLHRQNQYIJFFX-UHFFFAOYSA-K ytterbium(III) chloride Chemical compound [Cl-].[Cl-].[Cl-].[Yb+3] CKLHRQNQYIJFFX-UHFFFAOYSA-K 0.000 description 1
- 239000011592 zinc chloride Substances 0.000 description 1
- 235000005074 zinc chloride Nutrition 0.000 description 1
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
- C09K11/00—Luminescent, e.g. electroluminescent, chemiluminescent materials
- C09K11/02—Use of particular materials as binders, particle coatings or suspension media therefor
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y20/00—Nanooptics, e.g. quantum optics or photonic crystals
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y40/00—Manufacture or treatment of nanostructures
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
- C09K11/00—Luminescent, e.g. electroluminescent, chemiluminescent materials
- C09K11/08—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials
- C09K11/66—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials containing germanium, tin or lead
- C09K11/664—Halogenides
- C09K11/665—Halogenides with alkali or alkaline earth metals
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- Organic Chemistry (AREA)
- General Physics & Mathematics (AREA)
- Condensed Matter Physics & Semiconductors (AREA)
- Inorganic Chemistry (AREA)
- Optics & Photonics (AREA)
- Composite Materials (AREA)
- Biophysics (AREA)
- Life Sciences & Earth Sciences (AREA)
- Manufacturing & Machinery (AREA)
- Luminescent Compositions (AREA)
Abstract
本发明公开了一种高荧光量子产率紫光钙钛矿量子点的制备方法,包括如下步骤:1)将铯盐、有机配体以及非配位溶剂相混合,在惰性气体的保护下,加热获得铯离子前驱液;2)将氯化铅、氯盐添加剂、非配位溶剂相混合,在惰性气体的保护下,加热获得氯化铅前驱液;3)将铯前驱液加入到氯化铅前驱液中,获得紫光钙钛矿量子点溶液;4)通过液相配体交换工艺,对紫光钙钛矿量子点进行表面修饰;5)将步骤4)获得的粗溶液进行提纯,获得干净的紫光钙钛矿量子点产品。该方法制备出的紫光钙钛矿量子点尺寸均一、色纯度高、分散性好,荧光量子产率达90%以上,在空气中能够保持30天发光强度无衰减,为紫光QLEDs的应用提供材料基础。
Description
技术领域
本发明属于纳米功能材料制备技术领域,涉及一种钙钛矿量子点的制备方法,尤其涉及一种高荧光量子产率紫光钙钛矿量子点的制备方法。
背景技术
作为新型的发光二极管显示技术,有机物发光二极管(OLED第二代)和传统的II-VI和III-V族量子点发光二极管(QLEDs第三代)虽然可以产生紫光发光特性,然而由于材料的局限性,大多数制备的紫光LED显示出了宽的电致发光峰。为了降低紫光的发射线宽并提高色纯度,人们采用的滤光片,但这种方法会造成发光性能的浪费和器件显示效果的下降。作为一种新型的发光材料,铅卤钙钛矿量子点由于具有高的荧光量子产率,窄的半峰宽,成分与尺寸相关的荧光发射峰,这些优异发光特性使钙钛矿量子点从固态照明到全彩显示都有具大的应用潜力。自从全无机的钙钛矿量子点被首次报告以来,基于钙钛矿量子点的QLEDs的效率就逐渐的攀升,到目前为止,红、绿QLEDs器件的外量子效率(EQE)都先后超过了20%,展现出很好的商业应用价值;但蓝紫光钙钛矿量子点由于较宽的带隙和丰富的表面缺陷,以及钙钛矿八面体结构易受外界环境影响发生扭转而导致荧光强度损失,与红、绿钙钛矿量子点90%左右的荧光量子产率相比,紫光钙钛矿量子点的荧光量子产率低,发光强度弱,合成难度大,导致紫光QLEDs(< 435nm)的外量子效率仍然徘徊在0.1%左右,限制了钙钛矿量子点在显示领域的全色彩应用。
发明内容
为了提升紫光钙钛矿量子点荧光量子产率低的问题,本发明提出了一种高荧光量子产率紫光钙钛矿量子点的制备方法,通过加入不同种类氯盐,紫光量子点的氯空位得到一个很好的钝化,同时调节钙钛矿结构的容差因子,显著克服了钙钛矿结构正八面体的扭转,紫光钙钛矿量子点的荧光强度与荧光量产率得到了一个显著提升,最后通过功能配体的修饰,紫光钙钛矿量子点的稳定性以及分散性得到显著改善。
一种高荧光量子产率紫光钙钛矿量子点的制备方法,包括以下步骤:
1)将铯源、有机配体和非配位溶剂相混合,在80~150℃、真空度0.01~0.1MPa条件下,通入惰性气体搅拌反应60~180min,待溶液澄清透明后,获得铯前驱液;
铯源为硬脂酸铯、碳酸铯、硫酸铯、醋酸铯和草酸铯中的一种;有机配体为辛酸、油酸、硬脂酸、葵酸、三辛基氧膦中的一种或多种;非配位溶剂为十八烯、二十烯、辛烷、十六烯、十四烯、十二烷中的一种或多种;惰性气体为氮气或氩气;有机配体与非配位溶剂的体积比为0.02~0.8:1,铯源在有机配体和非配位溶剂构成的混合体系中质量浓度为1.5%~7.3%,铯前驱液的浓度为0.002~0.5g/mL。
2)将氯化铅、氯盐添加剂和非配位溶剂相混合,在100~150℃、真空度0.01~0.1MPa条件下,通入惰性气体反应0.5~2h,接着加入阴离子配体和阳离子配体并升温至150~240℃,待溶液澄清透明后,获得氯化铅前驱液;
非配位溶剂为十八烯、二十烯、辛烷、十六烯、十四烯、十二烷中的一种或多种,氯盐添加剂为氯化铷、氯化钾、氯化钠、氯化锂、稀土氯化盐(氯化铕、氯化钐、氯化铈、氯化铽、氯化镱)和氯化铁、氯化锰、氯化镍、氯化铜、氯化锌、氯化铟、氯化锶、氯化钙中的一种或多种,惰性气体为氮气或氩气中的一种,阳离子配体为油酸、硬脂酸、草酸、十一烯酸、月桂酸、乙酸、辛酸、三辛基氧膦中的一种或多种,阴离子配体为二己胺、油胺、三辛基磷、癸胺、叔丁胺、正丁胺、苯胺、萘胺、二辛基胺、辛胺中的一种或多种。氯化铅与氯盐添加剂的质量比为0.05~1.3:1,氯盐添加剂在非配位溶剂中的浓度为0.008~0.8g/mL,阳离子配体的添加量为0.005~0.4 mL/mL(固体0.0005~0.1 g/mL),阴离子配体的添加量为0.005~0.4 mL/mL(固体0.0005~0.1 g/mL),氯化铅前驱液的浓度0.005~0.4 g/mL。
3)将步骤1)中的铯前驱液加入到步骤2)中的氯化铅前驱液中,在80~240℃条件下搅拌反应5s~30min,然后迅速将混合溶液冷却至室温,获得钙钛矿量子点原液;铯前驱液与铅卤前驱液的体积比为0.02~0.5:1,冷却方式为冰水浴、液氮中的一种。
4)将功能配体加入到步骤3)所得钙钛矿量子点原液中,在25~150℃条件下搅拌反应0.2~24h,获得功能化钙钛矿量子点原液;
功能配体为三丁基膦、十二烷基苯磺酸、二苯基膦、双十二烷基二甲基溴化铵、5-氨基水杨酸、4-巯基丁酸、巯基丙酸、磺基甜菜碱、5-氨基戊酸、氨基酸中的一种或多种,对于1mL的钙钛矿量子点原液,功能配体的量为0.01~0.5mL,滴加速度为5 s~60min/mL。
5)将沉淀剂加至步骤4)所得功能化钙钛矿量子点原液中离心取沉淀,随后将沉淀加至溶剂中再分散,重复离心多次,最后获得尺寸均一、单分散的紫光钙钛矿量子点。对于1mL的功能化钙钛矿量子点原液,沉淀剂的添加量为0.3~5mL,沉淀剂和与溶剂的体积比为0.5~3:1,溶剂为甲苯、正己烷、环己烷、苯、辛烷中的一种,沉淀剂为乙酸甲酯、乙酸乙酯中的一种。
所述紫光钙钛矿量子点的浓度为5~150 mg/mL;量子点的粒径尺寸为3~100 nm,荧光峰位置在380~415nm,荧光量子产率为70%~95%;荧光寿命为0.1~500 ns。
综上,本发明具有如下优点:
1、首先通过在紫光钙钛矿量子点合成过程中添加金属氯化盐,一方面氯化盐在溶液中可以产生丰富的氯离子,很好的自钝化紫光钙钛矿量子点表面的氯空位,增强紫光钙钛矿量子点的荧光量子产率;另一方面通过二价金属元素的掺杂,改善了紫光钙钛矿量子点的容差因子,提高了紫光钙钛矿量子点的结构稳定性,同时还可以在本质上减少钙钛矿量子点中铅的含量,减缓毒性。最后利用功能配体对紫光钙钛矿量子点进行修饰,进一步提高紫光钙钛矿量子点的稳定性。
2、该方法制备出的紫光钙钛矿量子点尺寸均一、色纯度高、分散性好,荧光量子产率可达90%以上,在空气中能够保持30天发光强度几乎无任何衰减,同时制备工艺简单,成本低廉,可以大批量、高重复率的迅速制备,为高性能的紫光量子点发光二极光提供了很好的材料基础。
附图说明
图1为根据本发明的高荧光量子产率的紫光钙钛矿量子点的制备方法制备得到的Sr:CsPbCl3钙钛矿量子点的透射电镜形貌图;
图2为根据本发明的高荧光量子产率的紫光钙钛矿量子点的制备方法制备得到的Sr:CsPbCl3钙钛矿量子点的X射线衍射谱图;
图3为根据本发明的高荧光量子产率的紫光钙钛矿量子点的制备方法制备得到的Sr:CsPbCl3钙钛矿量子点的荧光图;
图4为根据本发明的高荧光量子产率的紫光钙钛矿量子点的制备方法制备得到的Sr:CsPbCl3钙钛矿量子点的吸收图;
图5为根据本发明的高荧光量子产率的紫光钙钛矿量子点的制备方法制备得到的Sr:CsPbCl3钙钛矿量子点的EDS能谱图;
图6为根据本发明的高荧光量子产率的紫光钙钛矿量子点的制备方法制备得到的Sr:CsPbCl3钙钛矿量子点荧光稳定性图。
具体实施方式
下面结合具体实施例对本发明做进一步的解释说明。
实施例1
本实施例为高荧光量子产率的紫光Sr:CsPbCl3量子点的制备方法,包括以下步骤:
1)将2.5mmol的碳酸铯加到15mL的十八烯中,同时加入1.25mL的油酸,然后抽气0.5小时,获得真空度为0.02MPa的无水无氧的环境,接着搅拌60分钟,待溶液澄清透明后,获得浓度为0.024 g/mL的铯前驱液;
2)将0.105g(0.38mmol)的氯化铅和0.1g氯化锶,同加入到10mL十八烯中,抽气0.5小时,获得真空度为0.02MPa的无水无氧的环境,随后升高温度至120℃,通入氮气反应时间为1小时,随后分别加入1mL油酸、1mL辛胺和2mL三辛基膦,接着升高温度至170℃,待溶液澄清透明后,获得浓度为0.015g/mL氯化铅前驱液;
3)将2mL的铯前驱液注入到10mL氯化铅前驱液中,在200℃反应30秒,接着将乙酸乙酯作为沉淀剂、甲苯作为溶剂离心Sr:CsPbCl3量子点,转速为8000rpm,离心时间为10min,最后将沉淀分散在无水甲苯中待用,获得提纯后Sr:CsPbCl3量子点分散液;
4)将0.02mL的巯基丙酸加入10 mL提纯后Sr:CsPbCl3量子点分散液中,常温搅拌6小时,搅拌速度为800rpm,获得巯基丙酸修饰的功能化Sr:CsPbCl3量子点原液;
5)乙酸乙酯作为沉淀剂、甲苯作为溶剂多次离心巯基丙酸修饰的功能化Sr:CsPbCl3量子点原液,每10mL功能化Sr:CsPbCl3量子点原液中乙酸乙酯的添加量30mL(每次10mL),乙酸乙酯与正己烷的体积比为1:1,转速为8000rpm,离心时间为5min,然后将沉淀分散在甲苯,获得干净的Sr:CsPbCl3量子点产品。
通过对Sr:CsPbCl3量子点进行TEM表征,发现产品是单分散,立方形的颗粒,尺寸为10nm(图1),并且具有较强的XRD衍射峰(图2),说明我们的方法合成的钙钛矿量子点结晶性良好,意味着更少的晶格缺陷,更高的荧光量子产率。
通过光谱表征发现,Sr:CsPbCl3量子点的荧光峰处于408nm,半峰宽高为12nm,吸收峰处于370nm,斯托克斯位移为12nm(图3-4),展示了优异的发光性能,可将其应用于QLEDs。
通过Sr:CsPbCl3量子点进行EDS表征,样品展示了很好的Cs、Pb、Cl、Sr元素特征峰(图5),说明我们成功制备了紫光Sr:CsPbCl3量子点。
最后将Sr:CsPbCl3量子点产品在空气中保持30天,发现其发光强度几乎无任何衰减(图6)。综上分析,说明我们成功的制备了高荧光量子产率、高稳定的紫光Sr:CsPbCl3量子点。
实施例2
本实施例为高荧光量子产率的紫光Cu:CsPbCl3量子点的制备方法,包括以下步骤:
1)将2mmol的碳酸铯加到15mL的十八烯中,同时加入2mL的油酸,然后抽气0.5小时,获得真空度为0.02MPa的无水无氧的环境,接着搅拌60分钟,待溶液澄清透明后,获得浓度为0.024 g/mL的铯前驱液;
2)将0.105g(0.38mmol)的氯化铅和0.08g氯化铜,同加入到10mL十八烯中,抽气0.5小时,获得真空度为0.02MPa的无水无氧的环境,随后升高温度至120℃,通入氮气反应时间为1小时,随后分别加入1mL油酸、1mL辛胺和2mL三辛基膦,接着升高温度至170℃,待溶液澄清透明后,获得0.013g/mL氯化铅前驱液;
3)将2mL的铯前驱液注入到10mL氯化铅前驱液中,在200℃反应30秒,接着将乙酸乙酯作为沉淀剂、甲苯作为溶剂离心Cu:CsPbCl3量子点,转速为8000rpm,离心时间为10min,最后将沉淀分散在无水甲苯中待用,获得提纯后Cu:CsPbCl3量子点分散液;
4)将10mg的4-巯基丁酸加入10mL提纯后Cu:CsPbCl3量子点中,80℃搅拌12小时,搅拌速度为800 rpm,获得4-巯基丁酸修饰的功能性Cu:CsPbCl3量子点;
5)乙酸乙酯作为沉淀剂、甲苯作为溶剂多次次离心Cu:CsPbCl3量子点,乙酸乙酯与正己烷的体积比为1:1,转速为8000 rpm,离心时间为5min,然后将沉淀分散在甲苯,获得干净的Cu:CsPbCl3量子点产品。
实施例3
本实施例为高荧光量子产率的紫光K:CsPbCl3量子点的制备方法,包括以下步骤:
1)将2mmol的碳酸铯加到15mL的十八烯中,同时加入2mL的油酸,然后抽气0.5小时,获得真空度为0.02MPa的无水无氧的环境,接着搅拌60分钟,待溶液澄清透明后,获得浓度为0.024 g/mL的铯前驱液;
2)将0.105g (0.38mmol)的氯化铅和0.05g氯化钾,同加入到10mL十八烯中,抽气0.5小时,获得真空度为0.02MPa的无水无氧的环境,随后升高温度至120℃,反应时间为1小时,接着通入氮气,随后分别加入1mL油酸、1mL油胺和2mL的三辛基膦,接着升高温度至220℃,待溶液澄清透明后,获得0.110g/mL氯化铅离子前驱液;
3)将2 mL的铯前驱液注入到10 mL的氯化铅离子前驱液中,在200℃反应30秒,接着将乙酸乙酯作为沉淀剂、甲苯作为溶剂离心K:CsPbCl3量子点,转速为8000 rpm,离心时间为10 min,最后将沉淀分散在无水甲苯中待用,获得K:CsPbCl3量子点分散液;
4)将3mg的5-氨基戊酸加入10mL提纯后K:CsPbCl3量子点分散液中,120℃搅拌12小时,搅拌速度为800rpm,获得5-氨基戊酸修饰的功能化K:CsPbCl3紫光量子点;
5)将乙酸乙酯作为沉淀剂、甲苯作为溶剂次离心功能化K:CsPbCl3紫光量子点,乙酸乙酯与正己烷的体积比为1:1,转速为6000rpm,离心时间为5min,然后将沉淀分散在甲苯,获得干净的Cu:CsPbCl3量子点产品。
实施例4
本实施例为高荧光量子产率的紫光Nd:CsPbCl3量子点的制备方法,包括以下步骤:
1)将2mmol的碳酸铯加到15mL的十八烯中,同时加入2mL的油酸,然后抽气0.5小时,获得真空度为0.02MPa的无水无氧的环境,接着搅拌60分钟,待溶液澄清透明后,获得浓度为0.024 g/mL的铯前驱液;
2)将0.105g (0.38mmol)的氯化铅和0.07g氯化钕,同加入到10mL十八烯中,抽气0.5小时,获得真空度为0.02MPa的无水无氧的环境,随后升高温度至120℃,反应时间为1小时,接着通入氮气,随后分别加入1mL油酸、1mL油胺和2mL的三辛基膦,接着升高温度至220℃,待溶液澄清透明后,获得0.025g/mL氯化铅离子前驱液;
3)将2 mL的铯前驱液注入到10 mL的氯化铅离子前驱液中,在200℃反应30秒,接着将乙酸乙酯作为沉淀剂、甲苯作为溶剂离心Nd:CsPbCl3量子点,转速为8000 rpm,离心时间为10 min,最后将沉淀分散在无水甲苯中待用,获得Nd:CsPbCl3量子点分散液;
4)将2mg的5-氨基水杨酸加入10mL提纯后Nd:CsPbCl3量子点分散液中,120℃搅拌12小时,搅拌速度为800rpm,获得5-氨基水杨酸修饰的功能化Nd:CsPbCl3紫光量子点;
5)将乙酸乙酯作为沉淀剂、甲苯作为溶剂次离心功能化Nd:CsPbCl3紫光量子点,乙酸乙酯与正己烷的体积比为2:1,转速为8000rpm,离心时间为5min,然后将沉淀分散在甲苯,获得干净的Nd:CsPbCl3量子点产品。
Claims (4)
1.一种高荧光量子产率紫光钙钛矿量子点的制备方法,其特征在于,包括以下步骤:
1)将铯源、有机配体和非配位溶剂相混合,在80~150℃、真空度0.01~0.1MPa条件下,通入惰性气体搅拌反应60~180min,待溶液澄清透明后,获得铯前驱液;
2)将氯化铅、氯盐添加剂和非配位溶剂相混合,在80~150℃、真空度0.01~0.1MPa条件下,通入惰性气体反应0.5~2h,接着加入阴离子配体和阳离子配体并升温至150~240℃,待溶液澄清透明后,获得氯化铅前驱液;
非配位溶剂为十八烯,氯盐添加剂为氯化锶,惰性气体为氮气或氩气中的一种,阳离子配体为油酸,阴离子配体为三辛基磷、辛胺中的一种或多种;
氯化铅与氯盐添加剂的质量比为1.05~1.3:1,氯盐添加剂在非配位溶剂中的浓度为0.008~0.8g/mL,阳离子配体的添加量为0.003~0.5mL/mL,阴离子配体的添加量为0.005~0.4 mL/mL,氯化铅前驱液的浓度0.005~0.4 g/mL;
3)将步骤1)中的铯前驱液加入到步骤2)中的氯化铅前驱液中,在100~240℃条件下搅拌反应5s~30min,然后迅速将混合溶液冷却至室温,获得钙钛矿量子点原液;
4)将功能配体加入到步骤3)所得钙钛矿量子点原液中,在25~150℃条件下搅拌反应0.2~24h,获得功能化钙钛矿量子点原液;功能配体为4-巯基丁酸、巯基丙酸中的一种或多种,对于1mL的钙钛矿量子点原液,功能配体的量为0.01~0.5mL;
5)将沉淀剂加至步骤4)所得功能化钙钛矿量子点原液中离心取沉淀,随后将沉淀加至溶剂中再分散,重复离心多次,最后获得尺寸均一、单分散的紫光钙钛矿量子点;
步骤1)中,有机配体与非配位溶剂的体积比为0.02~0.8:1,铯源在有机配体和非配位溶剂构成的混合体系中的质量浓度为1.5%~7.3%,铯前驱液的浓度为0.002~0.5g/mL;
步骤1)中,铯源为硬脂酸铯、碳酸铯、硫酸铯、醋酸铯和草酸铯中的一种;有机配体为油酸;非配位溶剂为十八烯;惰性气体为氮气或氩气;
所述高荧光量子产率紫光钙钛矿量子点的荧光量子产率为70%~95%。
2.如权利要求1所述一种高荧光量子产率紫光钙钛矿量子点的制备方法,其特征在于:步骤3)中,铯前驱液与铅卤前驱液的体积比为0.02~0.5:1,冷却方式为冰水浴、液氮中的一种。
3.如权利要求1所述一种高荧光量子产率紫光钙钛矿量子点的制备方法,其特征在于:步骤5)中,对于1mL的功能化钙钛矿量子点原液,沉淀剂的添加量为0.3~5mL,沉淀剂和与溶剂的体积比为0.5~3:1,溶剂为甲苯、正己烷、环己烷、苯、辛烷中的一种,沉淀剂为乙酸甲酯、乙酸乙酯中的一种。
4.如权利要求1所述一种高荧光量子产率紫光钙钛矿量子点的制备方法,其特征在于:所述紫光钙钛矿量子点的浓度为5~150 mg/mL;量子点的粒径尺寸为3~100 nm,荧光峰位置在380~415nm;荧光寿命为0.1~500 ns。
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